EP0608744B1 - Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments - Google Patents

Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments Download PDF

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Publication number
EP0608744B1
EP0608744B1 EP94100584A EP94100584A EP0608744B1 EP 0608744 B1 EP0608744 B1 EP 0608744B1 EP 94100584 A EP94100584 A EP 94100584A EP 94100584 A EP94100584 A EP 94100584A EP 0608744 B1 EP0608744 B1 EP 0608744B1
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EP
European Patent Office
Prior art keywords
spinning solution
filaments
cellulose acetate
degree
acetone
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP94100584A
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German (de)
English (en)
Other versions
EP0608744A1 (fr
Inventor
Ties Dipl.-Chem. Dr. Karstens
Wolfgang Dipl.-Ing. Koppe
Joachim Dipl.-Chem. Dr. Schätzle
Günter Dipl.-Ing. Maurer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cerdia Produktions GmbH
Original Assignee
Rhodia Acetow GmbH
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Publication date
Application filed by Rhodia Acetow GmbH filed Critical Rhodia Acetow GmbH
Publication of EP0608744A1 publication Critical patent/EP0608744A1/fr
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Publication of EP0608744B1 publication Critical patent/EP0608744B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
    • D01F2/30—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate by the dry spinning process
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/2964—Artificial fiber or filament
    • Y10T428/2965—Cellulosic

Definitions

  • the invention relates to filaments based on a cellulose acetate soluble in acetone, an optically isotropic spinning solution for the production of filaments, which is a cellulose acetate dissolved in acetone and optionally further additives contains, as well as the use of this spinning solution for the preparation of the designated Filaments.
  • DE-OS 27 05 382 describes an extensive group of cellulose derivatives, i.a. also cellulose acetates. These are said to be in an anisotropic spinning solution transferred to produce filaments using conventional spinning processes. According to Table I, the degree of substitution (DS) of the cellulose acetate between 1.89 to 2.45. Most suitable solvents are: halogenated and phenolic compounds specified. In connection with the other cellulose derivatives specified in DE-OS 27 05 382 Acetone is also listed in a large number of solvents. The cellulose derivatives in the spinning solution in an amount of at least 15 vol.% are available to meet the requirement for optical anisotropy.
  • DE-OS 27 05 382 In the DE-OS 27 05 382 is, however, the combination "cellulose acetate dissolved in acetone" not mentioned. And otherwise a 15 vol.% Acetone solution of the cellulose acetate described in DE-OS 27 05 382 also not optically anisotropic, but optically isotropic.
  • a cellulose acetate with a degree of substitution (DS) of 1.89 is not soluble in acetone.
  • DS degree of substitution
  • DE-OS 27 05 382 Cellulose derivatives with an average degree of polymerization (DP) of at least 100 anhydroglucose units have a sufficiently high molecular weight to be suitable for the production of filaments.
  • DE-OS 27 05 382 does not contain any precise statements on the degree of polymerization of the cellulose acetate or the degree of substitution between 1.89 and 2.45.
  • WO 94/06954 which belongs to the prior art according to Article 54 (3) EPC, discloses a method for spinning a solution in acetone of cellulose acetate with an intrinsic viscosity of preferably 1.35 (equal to a DP of 196) or more, and an acetyl content of 39.5% by weight (corresponds to a degree of substitution (DS) of 2.45).
  • the filaments have a titer of up to 1.56 dtex (1.4 denier) and contain a finely divided pigment (TiO 2 ) in amounts of less than 0.94% by weight.
  • An overall view of the prior art shows that in Connection with acetone as the solvent of a spinning solution of cellulose-2,5-acetate a high degree of polymerization of 300 is required, with the result that the spinning solution only has a low concentration of about 20 to 30% Has cellulose-2.5 acetate.
  • a starting material of this degree of polymerization can its concentration in acetone to produce a Spinning solution should not be raised further because it is inevitable sharp increase in the viscosity of the spinning solution is associated with that of usual Spinning devices can no longer be spun (for example at 40 to 50%).
  • a noticeably increased concentration would have the advantage offer that the content of acetone in the spinning solution can be drastically reduced could result in significant energy savings in circulation and recovery of acetone.
  • the invention is therefore based on the object of filaments on the basis of a cellulose acetate soluble in acetone and one especially for its production propose suitable spinning solution, which has the disadvantages described above the state of the art, especially the poor economy, fix without affecting the properties of the filaments, especially the tensile strength as well as the stretch, compared to known products become.
  • the above task is accomplished by filaments based on a soluble in acetone Dissolved cellulose acetate, which is characterized in that the degree of polymerization (DP) of the cellulose acetate is between 110 and 210. Especially the range of the degree of polymerization is preferred between 150 and 180 and especially between 160 and 180.
  • DP degree of polymerization
  • the degree of substitution (DS) is preferably set between 2.2 and 2.7. Especially it is preferred if the degree of substitution (DS) is between 2.4 and 2.6 and most preferably between 2.4 and 2.5.
  • the liter of filaments according to the invention is not critical. Preferably lies he between about 1 and 14 dtex, in particular between about 1.5 to 9 dtex. It is the fineness designation for filaments, i.e. a weight per length, the unit of which is the dtex.
  • the parameters of the filaments according to the invention are set in such a way that that their tensile strength between 0.9 and 1.2 cN / dtex, in particular between 1.0 and 1.2 cN / dtex, and the elongation between 10 and 30%, in particular between 15 and 25%. So they are enough the demands placed on the known filaments of this type, to make them suitable for the areas of application described below.
  • this optically isotropic spinning solution is characterized by that the concentration of cellulose-2,5-acetate in the spinning solution 35 to 47 mass% and the degree of polymerization (DP) of the cellulose-2,5-acetate is between 110 and 210. It is preferred here that the cellulose-2,5-acetate described above in connection with the Description of the filaments called degrees of polymerization and substitution having.
  • the optimal concentration of the cellulose-2,5-acetate in the invention optically isotropic spinning solution it is of particular advantage if its concentration (c) in the spinning solution is at most 8% by mass and in particular at most 6% by mass below the critical concentration (c *), measured at room temperature (approx. 20 ° C). Will this be critical Concentration of cellulose-2,5-acetate at higher concentrations of the spinning solution exceeded without the influence of external forces, such as shear forces (c> c *), then the spinning solution is converted from the isotropic to the anisotropic state.
  • optically isotropic spinning solution In order to further improve the optically isotropic spinning solution according to the invention, various additives can be incorporated, such as pigments and water.
  • the optically isotropic spinning solution according to the invention preferably contains up to 6% by mass and in particular 2 to 4% by mass of water. With the incorporation of water has the advantage that the viscosity of the Spinning solution reduced with the consequence of an improved spinnability becomes.
  • the spinning solution preferably contains one finely divided pigment, in particular a white pigment, such as preferably titanium dioxide.
  • the particle size is expediently in the range of about 0.3 ⁇ m to 0.5 ⁇ m.
  • the amount of fine pigment in the spinning solution is preferably 0.4 to 0.8 mass%, based on the proportion of Spinning solution on cellulose 2,5-acetate. The percentage by mass is very particularly preferred Range from about 0.4 to 0.6.
  • the advantages achievable with the invention can be described as follows:
  • the spinning mill can use an optically isotropic acetone spinning solution with a produce and spin a much higher content of cellulose-2,5-acetate, especially after the usual dry spinning.
  • filtertow In the preparation of from e.g. (Cigarettes) filtertow must be produced per unit of filtertow due to the high concentration of spinning solution much less acetone than can be recovered under the previous conditions. In this way can be, e.g. same filter tow production that with the recovery of the acetone associated costs markedly reduce.
  • the spinning mill based on the spinning solution according to the invention with the same viscosity Spinning solution produced and processed in a much higher concentration than before become.
  • the advantages mentioned above are accordingly with an optically isotropic acetone spinning solution high concentration of cellulose-2,5-acetate achieved.
  • the anisotropy or isotropy can be determined by visual inspection. An anisotropic phase looks cloudy and / or "pearly" while the isotropic phase is always clear.
  • the respective isotropic or anisotropic can also Condition of a spinning solution determined microscopically with crossed Nicols become. For example, if a sample of an anisotropic spinning solution between slide and cover glass of a microscope after pressing down of the coverslip observed between crossed Nicols is at least part of the solution is translucent.
  • the temperature also plays a role here a role; when the temperature of an anisotropic cellulose acetate solution of initially increased room temperature, then the anisotropic phase gradually change to the isotropic phase. If the temperature is increased further, the entire spinning solution is converted into an isotropic system.
  • the temperature ranges, at which these transitions take place vary depending on the type of Cellulose derivative, its concentration in the spinning solution and its Degree of substitution.
  • the possible uses of the filaments obtained according to the invention are not restricted compared to the known filaments of this type. So they can be used to manufacture filter tow (combined into a band Filament bundle), for tobacco smoke filters, especially cigarette filters, but also for example for the production of - textile - yarns for lining materials or of Blended fabrics with cotton can be used.
  • the starting point is an isotropic acetone solution of cellulose-2,5-acetate the designated species, their concentration close to the critical Concentration value (c *) can be raised, from which anisotropic Phase arises.
  • Such an isotropic solution will enter the spinneret channels (Capillaries) introduced, then cause those caused by the flow forces Shear forces in the spinneret channel that are predominantly an orientation and thus sets anisotropy.
  • the spinneret channels Capillaries
  • Fiber strengths In the area of the capillary and after exiting the isotropic phase from the capillary does not differ from a real one anisotropic phase. For this reason, you get almost the same in both cases Fiber strengths.
  • a spinning solution with the following composition was used: Dimensions-% Cellulose acetate (DP: 150; DS: 2.45) 43.2 water 3rd acetone 53.8
  • the spinning solution was spun in a conventional dry spinning system which had a nozzle plate with 125 nozzle channels.
  • the nozzle channels were triangular in cross section. The triangle had an edge length of 45 ⁇ m.
  • the nozzle temperature was 47 ° C and the nozzle pressure was 88 bar.
  • the spinning speed was 340 m / min with a draw factor of 1.6.
  • a temperature of 70 ° C prevailed in the spinning shaft with a total length of 4 m located under the spinneret. 10 m 3 of acetone-air mixture were suctioned off per hour.
  • the filaments obtained had the following physical properties: Titer 3.1 dtex tensile strenght 1.0 cN / dtex strain 19.4%
  • the 125 filaments obtained by the method of this example were combined into a filament bundle. 80 such filament bundles became one Cigarette filter tow (English: cigarette filter tow) summarized.
  • a spinning solution with the following composition was used: Dimensions-% Cellulose acetate (DP: 170; DS: 2.47) 42.1 water 3rd acetone 54.9
  • the spinning solution was spun on the same dry spinning system as in Example 1, but the nozzle plate had 240 nozzle channels.
  • the nozzle channels would be triangular in cross section.
  • the triangle had an edge length of 45 ⁇ m.
  • the nozzle temperature was adjusted to 52 ° C and the nozzle pressure was 80 bar.
  • the spinning speed was 310 m / min with a stretching factor of 1.3.
  • the temperature in the spinning shaft located under the spinneret with a total length of 4 m was 70 ° C. 10 m 3 of acetone-air mixture were suctioned off per hour.
  • the filaments obtained had the following physical properties: Titer 3.6 dtex tensile strenght 1.1 cN / dtex strain 20.5%

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)

Claims (17)

  1. Filaments à base d'un acétate de cellulose soluble dans l'acétone, ayant un degré de polymérisation (DP) compris entre 110 et 210, une résistance à la traction comprise entre 0,9 et 1,2 cN/dtex et un allongement compris entre 10 et 30 %.
  2. Filaments selon la revendication 1, caractérisés en ce que le degré de polymérisation (DP) est compris entre 150 et 180 et en particulier entre 160 et 180.
  3. Filaments selon la revendication 1 ou 2, caractérisés en ce que le degré de substitution (DS) de l'acétate de cellulose est compris entre 2,2 et 2,7.
  4. Filaments selon la revendication 3, caractérisés en ce que le degré de substitution (DS) de l'acétate de cellulose est compris entre 2,4 et 2,6 et en particulier entre 2,4 et 2,5.
  5. Filaments selon l'une des revendications précédentes, caractérisés en ce que leur titre est compris entre 1 et 14 dtex.
  6. Filaments selon la revendication 5, caractérisés en ce que leur titre est compris entre 1,5 et 9 dtex.
  7. Filaments selon au moins l'une des revendications précédentes 1 à 6, caractérisés en ce qu'ils contiennent un pigment finement divisé, en particulier en une proportion de 0,1 à 0,8 % en masse.
  8. Solution de filage optiquement isotrope pour la fabrication de filaments, contenant un acétate de cellulose dissous dans de l'acétone, ayant un degré de polymérisation (DP)compris entre 110 et 210, et éventuellement d'autres additifs, caractérisée en ce que la concentration de l'acétate de cellulose dans la solution de filage va de 35 à 47 % en masse.
  9. Solution de filage selon la revendication 8, caractérisée en ce que le degré de polymérisation de l'acétate de cellulose est compris entre 150 et 180 et en particulier entre 160 et 180.
  10. Solution de filage selon la revendication 8 ou 9, caractérisée en ce que le degré de substitution (DS) de l'acétate de cellulose est compris entre 2,2 et 2,7.
  11. Solution de filage selon la revendication 10, caractérisée en ce que le degré de substitution (DS) de l'acétate de cellulose est compris entre 2,4 et 2,6 et en particulier entre 2,4 et 2,5.
  12. Solution de filage selon au moins l'une des revendications précédentes 8 à 11, caractérisée en ce que la concentration de l'acétate de cellulose dans l'acétone se situe au maximum à 8 % en masse, en particulier au maximum à 6 % en masse au-dessous de la concentration critique (c*), mesurée à la température ambiante (aux environs de 20°C), au dépassement de laquelle, vers une plus forte concentration d'acétate de cellulose, la solution de filage, sans l'action de forces extérieures, passe de l'état isotrope à l'état anisotrope.
  13. Solution de filage selon au moins l'une des revendications précédentes 8 à 12, caractérisée en ce qu'elle contient jusqu'à environ 6 % en masse et en particulier de 2 à 4 % en masse d'eau.
  14. Solution de filage selon au moins l'une des revendications précédentes 8 à 13, caractérisée en ce qu'elle contient un pigment finement divisé.
  15. Solution de filage selon la revendication 14, caractérisée en ce qu'elle contient, en tant que pigment finement divisé, un pigment blanc, en particulier du dioxyde de titane.
  16. Solution de filage selon la revendication 14 ou 15, caractérisée en ce qu'elle contient de 0,4 à 0,8 % en masse, par rapport à l'acétate de cellulose dans la solution de filage, de pigment finement divisé.
  17. Utilisation de la solution de filage selon au moins l'une des revendications 8 à 16, pour la fabrication de filaments selon au moins l'une des revendications 1 à 7, par filage à sec usuel.
EP94100584A 1993-01-26 1994-01-17 Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments Expired - Lifetime EP0608744B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4302055A DE4302055C1 (de) 1993-01-26 1993-01-26 Celluloseacetat-Filamente sowie ein Verfahren zu deren Herstellung
DE4302055 1993-01-26

Publications (2)

Publication Number Publication Date
EP0608744A1 EP0608744A1 (fr) 1994-08-03
EP0608744B1 true EP0608744B1 (fr) 1999-03-31

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EP94100584A Expired - Lifetime EP0608744B1 (fr) 1993-01-26 1994-01-17 Filaments d'acétate de cellulose, solution de filage optiquement isotrope à cet effet et son utilisation pour la fabrication des filaments

Country Status (11)

Country Link
US (1) US5449555A (fr)
EP (1) EP0608744B1 (fr)
JP (1) JP2950490B2 (fr)
KR (1) KR960011600B1 (fr)
CN (1) CN1100478A (fr)
AT (1) ATE178368T1 (fr)
BR (1) BR9400301A (fr)
CA (1) CA2113142A1 (fr)
DE (2) DE4302055C1 (fr)
ES (1) ES2131594T3 (fr)
RU (1) RU2085629C1 (fr)

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JP3342763B2 (ja) * 1994-02-04 2002-11-11 ダイセル化学工業株式会社 シガレットフィルター素材
DE69509982T2 (de) * 1994-03-01 2000-01-27 Kuraray Co Mit dispergierfarbstoff faerbbare regenierte zellulosefaser und diese enthaltendes textilprodukt
EP0706766B1 (fr) * 1994-09-22 2002-08-14 Daicel Chemical Industries, Ltd. Matériau filtrant pour la fumée de tabac et son procédé de fabrication
US5491024A (en) * 1995-03-14 1996-02-13 Hoechst Celanese Corporation Photodegradable cellulose ester tow
JP3942669B2 (ja) * 1995-03-31 2007-07-11 ダイセル化学工業株式会社 物理強度に優れたセルロースアセテート、及びその製造法
WO1996030413A1 (fr) * 1995-03-31 1996-10-03 Daicel Chemical Industries, Ltd. Acetate de cellulose a bonne aptitude au moulage et procede de preparation associe
US5914397A (en) * 1995-03-31 1999-06-22 Daicel Chemical Industries, Ltd. Cellulose acetate excellent in physical strength, and process for production thereof
DE19730485C2 (de) * 1997-07-16 2003-07-03 Rhodia Acetow Ag Celluloseacetatfilamente mit trilobalem Querschnitt
US8039531B2 (en) 2003-03-14 2011-10-18 Eastman Chemical Company Low molecular weight cellulose mixed esters and their use as low viscosity binders and modifiers in coating compositions
US7585905B2 (en) 2003-03-14 2009-09-08 Eastman Chemical Company Low molecular weight cellulose mixed esters and their use as low viscosity binders and modifiers in coating compositions
US8461234B2 (en) 2003-03-14 2013-06-11 Eastman Chemical Company Refinish coating compositions comprising low molecular weight cellulose mixed esters
US8124676B2 (en) 2003-03-14 2012-02-28 Eastman Chemical Company Basecoat coating compositions comprising low molecular weight cellulose mixed esters
GB2504495A (en) * 2012-07-30 2014-02-05 British American Tobacco Co Fleece for smokeless tobacco pouch
RU2515313C2 (ru) * 2012-08-27 2014-05-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тюменский государственный нефтегазовый университет" (ТюмГНГУ) Способ модификации диацетатцеллюлозных волокон

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Publication number Publication date
JP2950490B2 (ja) 1999-09-20
CA2113142A1 (fr) 1994-07-27
ATE178368T1 (de) 1999-04-15
DE59408019D1 (de) 1999-05-06
JPH06280107A (ja) 1994-10-04
US5449555A (en) 1995-09-12
KR940018496A (ko) 1994-08-18
EP0608744A1 (fr) 1994-08-03
RU2085629C1 (ru) 1997-07-27
BR9400301A (pt) 1994-08-16
CN1100478A (zh) 1995-03-22
KR960011600B1 (ko) 1996-08-24
ES2131594T3 (es) 1999-08-01
DE4302055C1 (de) 1994-03-24

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